CN101830696A - Dielectric ceramic composition and electronic unit - Google Patents

Dielectric ceramic composition and electronic unit Download PDF

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CN101830696A
CN101830696A CN201010116971A CN201010116971A CN101830696A CN 101830696 A CN101830696 A CN 101830696A CN 201010116971 A CN201010116971 A CN 201010116971A CN 201010116971 A CN201010116971 A CN 201010116971A CN 101830696 A CN101830696 A CN 101830696A
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ceramic composition
dielectric ceramic
oxide compound
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principal constituent
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梅田裕二
张帆
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TDK Corp
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TDK Corp
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Abstract

The invention provides dielectric ceramic composition, it has principal constituent and minor component, and described principal constituent contains useful composition formula (Sr xBa 1-x) mTiO 3The compound of (0.159≤x≤0.238,0.997≤m≤1.011) expression, described minor component has: the CaTiO of 11～25 weight % 3, be converted into FeO 3/2, CoO 4/3, NiO, CuO and ZnO be 0.10～0.50 weight % be selected among Fe, Co, Ni, Cu and the Zn more than one oxide compound, be scaled the oxide compound (A is Mn and/or Cr) of the A element of 0.590～1.940 mole of % and the oxide compound (D is selected from more than a kind of La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho and Y) of D element with element, the mol ratio (A/D) of D element and A element is 2.250～7.450.According to the present invention, can provide not contain Pb and Bi, can reduce dielectric loss at wide frequency field, and the dielectric ceramic composition of capacity temperature characteristic and specific inductivity excellence.

Description

Dielectric ceramic composition and electronic unit
Technical field
The present invention relates to the dielectric ceramic composition that in the dielectric layer of electronic unit etc., uses.And then at length, relate to dielectric ceramic composition and the electronic unit that uses it, described dielectric ceramic composition does not contain as lead of carrying capacity of environment material (Pb) and the surging bismuth (Bi) of resource price, dielectric loss is reduced, and then higher dielectric constant arranged, the simultaneous temperature characteristic is relatively good, and can provide with cheap price.
Background technology
In recent years, the environment protection campaign of earth scale grows to even greater heights, and in the field of electronic unit, also require to reduce the carrying capacity of environment material of plumbous (Pb) etc.Therefore, people expect exploitation not leaded (Pb), and the dielectric ceramic composition with the above characteristic of same degree.
In addition, constitute the miniaturization, complicated developed of the circuit of electronic machine etc., therefore for the electronic unit that carries on circuit, except further miniaturization, also because in order to prevent the former of mishandle etc. thereby to require himself heating few.Therefore, the ceramic condenser for as an example of electronic unit also requires it can keep good temperature profile, simultaneously in order to adapt with miniaturization and to improve specific inductivity, and requires low dielectric loss for the reduction of self-heating.
On the other hand, in recent years, because resource price is sharply surging, the manufacturing cost that contains the electronic unit of rare earth element is also raising, but electronic unit is owing to be used in the electronic machine in a large number, thereby requires it to keep high-performance, keeps low price simultaneously.
Especially, bismuth (Bi) is a kind of of the surging rare earth element of price in recent years, and it becomes the obstacle that reduces the electronic unit price.In addition, bismuth is evaporation easily in burning till (baked one-tenth), becomes the deviation of characteristic or the reason of the stove material deterioration in the firing furnace.
Therefore,, obtain the electronic unit of high characteristic simultaneously, require a kind of not only not leadedly, nor contain the dielectric ceramic composition of bismuth in order to take into account global environment protection and to reduce price.
For example, in Japan speciallyyed permit No. 3767377 communique, it was good to disclose temperature profile, and at the little dielectric ceramic composition of high-frequency region dielectric loss.But this dielectric ceramic composition contains Pb, with global environment protection require incompatible.
As the dielectric ceramic composition of not leaded (Pb), for example TOHKEMY 2003-238240 communique discloses by containing BaCO 3, Bi 2O 3And TiO 2Principal constituent in add among La, Nd, Ce, Sn, Zr, Ta, the Nb more than a kind and the dielectric ceramic composition that obtains.But the dielectric loss when 1MHz that this dielectric ceramic composition showed also is high under best situation, is about 0.1 (10%), can not suppress self-heating fully.Therefore, this dielectric ceramic composition miniaturization of adaptive circuit, complicated effectively in the mesohigh purposes.
And this dielectric ceramic composition contains bismuth, can not adapt to the requirement that reduces price.
Summary of the invention
The present invention is the invention of making in view of such present situation, its purpose is to provide reliably dielectric ceramic composition, this dielectric ceramic composition can be used for the dielectric layer of electronic units such as ceramic condenser, do not contain lead (Pb) and bismuth (Bi), dielectric loss is descended, and capacity temperature characteristic and relative permittivity (lead Bi Lure Electricity) excellence.In addition, the object of the present invention is to provide the electronic unit that uses this dielectric ceramic composition to obtain.
The inventor has carried out making great efforts research to achieve these goals, found that, even do not contain Pb and Bi, by making the specific composition of consisting of of dielectric ceramic composition, and the ratio that makes them is in specialized range, also can realize above-mentioned purpose, thereby finish the present invention.
That is, dielectric ceramic composition of the present invention is characterised in that it has principal constituent and minor component, and described principal constituent contains useful composition formula (Sr xBa 1-x) mTiO 3Expression and to satisfy x in the above-mentioned composition formula be that m in 0.159≤x≤0.238, the above-mentioned composition formula is the compound of 0.997≤m≤1.011 this relations, described minor component has: CaTiO 3, be selected from least a oxide compound among Fe, Co, Ni, Cu and the Zn, A element (Acceptor) oxide compound (wherein, A is selected from least a among Mn and the Cr) and the oxide compound of D element (Donor) is (wherein, D is selected from least a among La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho and the Y), with respect to above-mentioned principal constituent 100 weight %, contain 11～25 weight %CaTiO 3, be converted into FeO 3/2, CoO 4/3, NiO, CuO and ZnO be at least a oxide compound among Fe, Co, Ni, Cu and the Zn of being selected from of 0.10～0.50 weight %, with respect to 100 moles of % of above-mentioned principal constituent, contain and be converted into the Mn element and the Cr element is the oxide compound of the A element of 0.590～1.940 mole of %, above-mentioned A element is 2.250～7.450 with the ratio (A/D) of above-mentioned D element with molar ratio computing.
Dielectric ceramic composition of the present invention does not contain lead (Pb) and bismuth (Bi) in fact.But, even do not contain lead and bismuth, be above-mentioned composition and content by making principal constituent and minor component, also can access when can keep relative permittivity and temperature profile, at the few dielectric ceramic composition of wide frequency field dielectric loss.
According to the present invention, can provide electronic unit with the dielectric layer that constitutes with above-mentioned dielectric ceramic composition.Electronic unit of the present invention is not limited especially, can enumerate the mesohigh electrical condenser that for example in buffer circuit, uses.
According to the present invention, can provide supply unit with above-mentioned electronic unit.Supply unit of the present invention can be enumerated the supply unit that for example has buffer circuit.Supply unit of the present invention is owing to have above-mentioned electronic unit, and therefore heating is few.
Dielectric ceramic composition of the present invention, making its principal constituent and minor component is above-mentioned each composition, and then makes the scope of each components in proportions at afore mentioned rules, and does not contain lead (Pb) and bismuth (Bi).Consequently can reduce load, simultaneously can reduce dielectric loss, and can obtain capacity temperature characteristic excellence, dielectric ceramic composition that relative permittivity is high low price at wide frequency field for environment.
By in the dielectric layer of electronic units such as ceramic condenser, using this dielectric ceramic composition of the present invention, not leaded (Pb) and bismuth (Bi) can be provided, can dielectric loss be suppressed at low degree at wide frequency field, and capacity temperature characteristic and relative permittivity good electron parts.Therefore, the supply unit with electronic unit of the present invention can be realized low heating.
Description of drawings
[Fig. 1] Figure 1A is the front elevation of the ceramic condenser of one embodiment of the present invention, and Figure 1B is the side cross-sectional view of the ceramic condenser of one embodiment of the present invention.
Embodiment
Below, based on embodiment explanation the present invention shown in the drawings.
Ceramic condenser 2
Shown in Figure 1A, Figure 1B; the ceramic condenser 2 of present embodiment forms following structure; promptly; the pair of terminal electrode (terminal Electricity Very) 12,14 that has dielectric layer 10, forms its apparent surface; with the pin 6,8 that is connected on this terminal electrode 12,14, cover them with protection resin 4.The shape of ceramic condenser 2 can suitably determine that preferred dielectric layer 10 forms the electrical condenser of the rondelle of circular plate shape according to purpose or purposes.In addition, its size can suitably determine that usually, diameter is about 5～20mm, is preferably about 5～15mm according to purpose or purposes.
Dielectric layer 10
Dielectric layer 10 contains dielectric ceramic composition of the present invention.Dielectric ceramic composition of the present invention does not contain lead (Pb) and bismuth (Bi) in fact, has principal constituent and minor component, and described principal constituent contains useful composition formula (Sr xBa 1-x) mTiO 3The compound of expression, described minor component has CaTiO 3, be selected from least a kind oxide compound among Fe, Co, Ni, Cu and the Zn, A element oxide compound (wherein, A is at least a kind that is selected among Mn and the Cr) and the oxide compound (wherein, D is at least a kind that is selected among La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho and the Y) of D element.
Dielectric ceramic composition of the present invention is considered from the angle of above-mentioned environment and resource price, is not contained lead (Pb) and bismuth (Bi) in fact.The meaning that " does not contain in fact " is if be the amount of impurity level, also can contain lead (Pb) and bismuth (Bi) so in dielectric ceramic composition of the present invention.For example, as the amount of impurity level, below 300ppm.
In addition, for the usefulness composition formula (Sr that in principal constituent, contains xBa 1-x) mTiO 3The compound of expression, the x in the composition formula is 0.159≤x≤0.240, preferred 0.170≤x≤0.233, more preferably 0.175≤x≤0.220.
X represents the ratio of Sr, when x too hour, the peaked ε max of the volume change rate in expression institute fixed temperature zone becomes excessive, and the tendency that can not meet the desired capacity temperature characteristic is arranged.When x is too big, the tendency that has capacity temperature characteristic to worsen.
In addition, the m in the above-mentioned composition formula is 0.997≤m≤1.011, preferred 0.999≤m≤1.008.
M represent Sr and Ba, with the mol ratio of Ti, when m too hour, the tendency that has dielectric loss to worsen.When m was too big, ε max became excessive, and the tendency that can not meet the desired capacity temperature characteristic is arranged.
Dielectric ceramic composition of the present invention contain oxide compound, the D element of A element oxide compound, be selected from least a kind oxide compound and CaTiO among Fe, Co, Ni, Cu and the Zn 3As minor component.
The oxide compound of A element has the effect that insulation resistance is increased.A element (Acceptor) is preferably Mn for being selected from least a kind among Mn and the Cr.With respect to 100 moles of % of above-mentioned principal constituent, the content of above-mentioned oxide compound is converted into MnO and CrO 3/2Be 0.590～1.940 mole of %, be preferably 0.779～1.753 mole of %, more preferably 0.876～1.460 mole of %.When content too after a little while, the tendency that has capacity temperature characteristic to worsen.On the other hand, when content too for a long time, the tendency that has dielectric loss and ε max to worsen.
And, for example when containing the oxide compound of Mn,, can use MnO as raw material, also can use MnCO 3In the dielectric ceramic composition after burning till, contain with the form of MnO.
The oxide compound of D element has the effect that reduces dielectric loss.D element (Donor) is selected from least a kind among La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho and the Y, is preferably Ce, La, Pr, Nd, Sm, more preferably Ce, La, Pr.
In the present invention, the ratio (A/D) of above-mentioned A element and D element is 2.250～7.450 with molar ratio computing, is preferably 2.990～6.740.By A/D being controlled at above-mentioned scope, can keep good relative permittivity and dielectric loss, meet the desired capacity temperature characteristic simultaneously.When A/D too hour, the tendency that has capacity temperature characteristic to worsen.On the other hand, when too big, the tendency that has dielectric loss and ε max to worsen.
At least a kind the oxide compound that is selected among Fe, Co, Ni, Cu and the Zn can improve capacity temperature characteristic, also has the effect that improves coking property.Be preferably the oxide compound of Zn, Fe, Ni, be preferably the oxide compound of Zn especially.The content of above-mentioned oxide compound is converted into FeO with respect to principal constituent 100 weight % 3/2, CoO 4/3, NiO, CuO and ZnO, be 0.10～0.50 weight %, be preferably 0.15～0.50 weight %, more preferably 0.20～0.45 weight %.If the content of these oxide compounds is too few, the tendency that then has dielectric loss to worsen.On the contrary, if the content of these oxide compounds is too much, the tendency that then has relative permittivity significantly to reduce.
CaTiO 3Effect with the temperature variation planarization that makes specific inductivity.CaTiO 3Content be 11～25 weight % with respect to principal constituent 100 weight %, be preferably 11～20 weight %, more preferably 12～17 weight %.Work as CaTiO 3Content when very few, the tendency that has dielectric loss to worsen, ε max becomes excessive simultaneously, and the tendency that can not meet the desired capacity temperature characteristic is arranged.Work as CaTiO 3Content when too much, the situation that has relative permittivity to reduce.
Thickness to dielectric layer 10 does not limit especially, can be preferably 0.3～2mm according to suitably decisions such as purposes.Thickness by making dielectric layer 10 goes for the mesohigh purposes in such scope.
Terminal electrode 12,14
Terminal electrode 12,14 usefulness electro-conductive materials constitute.The electro-conductive material that uses in the terminal electrode 12,14 for example contains Cu, Cu alloy, Ag, Ag alloy, In-Ga alloy etc. as principal constituent.In addition, terminal electrode 12,14 can be the single layer structure of these metal or alloy, also can be multilayered structure.
The manufacture method of ceramic condenser
Then, the manufacture method for the ceramic condenser of present embodiment describes.At first, be manufactured on the dielectric ceramic composition powder that burns till back formation dielectric layer 10 as shown in Figure 1.
At first, prepare the raw material of principal constituent and the raw material of minor component.The raw material of principal constituent can be enumerated each oxide compound of Sr, Ba, Ti and/or by burning till the raw material that forms these oxide compounds or their composite oxides etc., for example can use SrCO 3, BaCO 3Deng oxycarbide, TiO 2Deng oxide compound.In addition, the raw material of principal constituent can be made by solid phase method, also can make by the liquid phase method of hydrothermal synthesis method or oxalate method etc., but consider from the angle of manufacturing cost, preferably makes by solid phase method.
The raw material of minor component is limited especially the oxide compound of above-mentioned each minor component or composite oxides or can be from for example suitably selecting to use carbonate, nitrate, oxyhydroxide, the organometallic compound etc. by burning till all cpds that forms these oxide compounds or composite oxides.
Then, cooperate the raw material of principal constituent, forming the composition of afore mentioned rules, and use ball mill etc. to carry out wet mixing.The gained mixture is carried out granulation, moulding, in air atmosphere, the forming composition that obtains is calcined, can obtain the calcining powder of the raw material of principal constituent thus.Then, gained is calcined powder carry out coarse reduction, and then add the raw material of the minor component of specified amount, carry out wet mixing, form the dielectric ceramic composition powder.As calcination condition, for example calcining temperature is preferably 900～1200 ℃, and calcination time is preferably 0.5～4 hour.And, the raw material of the raw material of principal constituent and minor component can be calcined under identical conditions and be obtained the dielectric ceramic composition powder, also can with the raw material of the raw material of principal constituent and minor component after calcining under the different conditions, mix obtaining the dielectric ceramic composition powder.As mentioned above, prepare the dielectric ceramic composition powder, can realize desired characteristics, seek the reduction of manufacturing cost simultaneously by utilizing solid phase method.
Then, use tackiness agent etc. that gained dielectric ceramic composition powder is carried out granulation, and the granulation thing that obtains is shaped to has the discoideus of prescribed level, form thus and give birth to formed body (グ リ-Application molding).Burn till by gained is given birth to formed body, obtain dielectric ceramic composition as sintered compact.And, the condition of burning till is limited especially, but keep temperature to be preferably 1100～1400 ℃, more preferably 1150～1350 ℃, and preferably to burn till atmosphere be in air.
On the major surfaces of the sintered compact of gained dielectric ceramic composition, print terminal electrode, toast (the baked I is paid け) as required, form terminal electrode 12,14 thus.Then, utilize soldering etc. on terminal electrode 12,14, to engage pin 6,8, by with protection resin 4 cladding element bodies, obtain the single panel type ceramic condenser shown in Figure 1A, Figure 1B at last.
The ceramic condenser of the present invention of Zhi Zaoing is assembled in the buffer circuit in the switch power supply for example by pin 6,8 like this, can obtain supply unit of the present invention.
More than, be illustrated for embodiments of the present invention, but the present invention is not subjected to any restriction of these embodiments, in the scope that does not break away from purport of the present invention, can implement in various mode, this is mathematical.
For example, in the above-described embodiment, enumerated the single panel type ceramic condenser as electronic unit of the present invention, but electronic unit of the present invention is not limited to the single panel type ceramic condenser, also can be to use the laminated ceramic capacitor dielectric paste that contains above-mentioned dielectric ceramic composition powder and electrode paste, that make by common print process or slice method (シ one ト method).
Embodiment
Below, further the present invention is described, but the present invention is not limited to these embodiment based on detailed embodiment.
Embodiment
At first, as the principal constituent raw material, prepare SrCO respectively 3, BaCO 3And TiO 2And then, as the minor component raw material, prepare CaTiO 3, the A element oxide compound or carbonate (MnCO 3, Cr 2O 3), CuO, Fe 2O 3, Co 3O 4, NiO, ZnO, D element oxide compound (wherein, D is La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho and Y).And, CaTiO 3Prepare as described below.At first, with CaCO 3Raw material and TiO 2Raw material carries out wet mixing, and with dried raw material in air, calcine with 1000 ℃, 2 hours condition.Raw material after the calcining is further carried out case of wet attrition, thereby obtain CaTiO 3
Then, the raw material of difference weighing principal constituent, with the composition shown in the formation table 1, and by making water carry out wet mixing as the ball mill of solvent.Then, the gained mixture carried out drying after, the water that adds 5 weight % carries out granulation, moulding.With the gained forming composition in air, calcine with 1150 ℃, 2 hours condition.After carrying out coarse reduction with the powder of masher (ら い か い Machine) after, and then respectively weighing, add the raw material of minor component, make to reach the composition shown in the table 1, and carry out case of wet attrition calcining.By being dried, obtain having the dielectric ceramic composition powder that as shown in table 1 each formed (sample number into spectrum is each composition of 1～43).And, MnCO 3Form with MnO after burning till contains in dielectric ceramic composition.
Table 1
Figure GSA00000023745800081
" * " represents comparative example of the present invention.
Then, with respect to the dielectric ceramic composition powder that obtains: 100 weight %, add polyvinyl alcohol water solution: 10 weight %, carry out granulation then, and pass through screen cloth.Then, by with gained granulation powder 3t/cm 2Pressure carry out moulding, obtaining diameter is the discoideus living formed body that 16.5mm, thickness are about 1.2mm.
Then, in air, burn till, obtain discoideus sintered compact by the living formed body that will obtain with 1240 ℃, 2 hours condition.Coating Ag electrode on the major surfaces of the sintered compact that obtains, and then in air, under 800 ℃ the condition, carry out 10 minutes baking processing, obtain the sample (sample number into spectrum is 1～43) of discoideus ceramic condenser shown in Figure 1 thus.The thickness of the dielectric layer 10 of the capacitor sample that obtains is about 1mm.For each capacitor sample that obtains, utilize following method, respectively relative permittivity, dielectric loss, capacity temperature characteristic and insulation resistance are estimated.
Relative permittivity ε
Relative permittivity ε (no unit) is calculated by electrostatic capacity, described electrostatic capacity is for capacitor sample, under 25 ℃ reference temperature, utilizing digital LCR meter (the system 4274A of YHP society) is 1kHz in frequency, and incoming signal level (mensuration voltage) is to measure under the condition of 1.0Vrms.Preferred relative permittivity height is in the present embodiment, good with being designated as more than 1800.
Dielectric loss (tan δ)
Dielectric loss (tan δ) is for capacitor sample, under 25 ℃ reference temperature, utilizes digital LCR meter (the system 4274A of YHP society), is 1kHz and 100kHz in frequency, and incoming signal level (mensuration voltage) is to measure under the condition of 1.0Vrms.The preferable medium loss is low, in the present embodiment, during with the frequency of 1kHz be below 0.6%, during the frequency of 100kHz be designated as below 0.5% good.
Capacity temperature characteristic
For capacitor sample, measure electrostatic capacity-25～140 ℃ temperature ranges, the velocity of variation (unit is %) of the electrostatic capacity of the electrostatic capacity when calculating-25 ℃ and 125 ℃ during with respect to+25 ℃.In the present embodiment, the situation of volume change rate in+15%～-30% scope is designated as well.And, in the table 2 shown in following ,-25 ℃ volume change rates are expressed as Δ C (25)/C, 125 ℃ volume change rates are expressed as Δ C (125)/C.
Insulation resistance
Apply the volts DS of 500V for capacitor sample, measure insulation resistance.Preferred insulation resistance IR (unit is Ω) is big, in the present embodiment, and with 1 * 10 4Be designated as good more than the M Ω.
Table 2
Figure GSA00000023745800101
" * " represents comparative example of the present invention.
By table 1 and 2 as can be known, when the composition of dielectric ceramic composition within the scope of the invention when (sample number into spectrum be 2～7,10～12,15～17,20～21a, 24～27,29～43), satisfying relative permittivity is more than 1800, dielectric loss (1kHz) is below 0.6%, dielectric loss (100kHz) is below 0.5%, and insulation resistance is 1 * 10 4More than the M Ω, be+15%～-30% in the volume change rate of-25 ℃～125 ℃ four corners with respect to 25 ℃.
Promptly, can confirm that the composition by making dielectric ceramic composition can not contain lead (Pb) and bismuth (Bi) within the scope of the invention, and keep capacity temperature characteristic and relative permittivity well, be reduced in the dielectric loss (tan δ) of wide frequency field simultaneously.
With respect to this, can confirm composition when dielectric ceramic composition outside scope of the present invention when (sample number into spectrum 1,8,9,13,14,18,19,22,23,28), at least 1 person's variation of relative permittivity, dielectric loss (1kHz, 100kHz), insulation resistance, capacity temperature characteristic.

Claims (3)

1. dielectric ceramic composition is characterized in that, has principal constituent and minor component, and described principal constituent contains useful composition formula (Sr xBa 1-x) mTiO 3Represent and satisfy the compound of following relation: the x in the above-mentioned composition formula is that the m in 0.159≤x≤0.238, the above-mentioned composition formula is 0.997≤m≤1.011,
Described minor component has:
CaTiO 3、
Be selected from least a oxide compound among Fe, Co, Ni, Cu and the Zn,
The oxide compound of A element, wherein the A element be selected among Mn and the Cr at least a kind and
The oxide compound of D element, wherein the D element is at least a kind that is selected among La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho and the Y,
With respect to above-mentioned principal constituent 100 weight %, contain 11～25 weight %CaTiO 3, be converted into FeO 3/2, CoO 4/3, NiO, CuO and ZnO be at least a oxide compound among Fe, Co, Ni, Cu and the Zn of being selected from of 0.10～0.50 weight %,
With respect to 100 moles of % of above-mentioned principal constituent, contain and be converted into the Mn element and the Cr element is the oxide compound of the above-mentioned A element of 0.590～1.940 mole of %,
Above-mentioned A element is 2.250～7.450 with the ratio (A/D) of above-mentioned D element with molar ratio computing.
2. electronic unit, it has the dielectric layer that constitutes with the described dielectric ceramic composition of claim 1.
3. supply unit, it has the described electronic unit of claim 2.
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